CA1052538A - Apparatus for continuous liquid-liquid extraction of water with a solvent - Google Patents
Apparatus for continuous liquid-liquid extraction of water with a solventInfo
- Publication number
- CA1052538A CA1052538A CA219,738A CA219738A CA1052538A CA 1052538 A CA1052538 A CA 1052538A CA 219738 A CA219738 A CA 219738A CA 1052538 A CA1052538 A CA 1052538A
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- CA
- Canada
- Prior art keywords
- water
- solvent
- extraction vessel
- container
- extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Extraction Or Liquid Replacement (AREA)
Abstract
Inventors: BJORN OLOF JOSEFSSON
MARTIN AHNOFF
Title: APPARATUS FOR CONTINUQUS LIQUID-LIQUID
EXTRACTION OF WATER WITH A SOLVENT.
Abstract: An apparatus for extracting dissolved substances from water by means of a solvent comprises an extraction vessel, a mixing pontainer, open at the top, in the lower portion the extraction vessel and stirring means in said mixing con-tainer. The extraction vessel contains a desired quantity of solvent. The water is added in a continuous flow and is mixed with the solvent. The lighter solvent phase rises to the top of the apparatus, while the heavier water phase is continuously withdrawn through an annular space between the mixing container and the wall of the extraction vessel.
MARTIN AHNOFF
Title: APPARATUS FOR CONTINUQUS LIQUID-LIQUID
EXTRACTION OF WATER WITH A SOLVENT.
Abstract: An apparatus for extracting dissolved substances from water by means of a solvent comprises an extraction vessel, a mixing pontainer, open at the top, in the lower portion the extraction vessel and stirring means in said mixing con-tainer. The extraction vessel contains a desired quantity of solvent. The water is added in a continuous flow and is mixed with the solvent. The lighter solvent phase rises to the top of the apparatus, while the heavier water phase is continuously withdrawn through an annular space between the mixing container and the wall of the extraction vessel.
Description
i(~5Z538 The present invention relates to an apparatus for enriching chemicals in water by means of continuous liquid-liquid extraction in an extraction vessel with mechanical stirring.
~he increasing concentration of chemicals menacing the environment in our waterways necessitates substantially continuous supervision of the content of certain chemicals such as oil and chlorinated hydrocarbon, particularly polychlorinated biphenyls (PCB). The presence of such chemicals in lakes and rivers causes undesirable biological results, and careful supervision of their content is therefore necessary. Since these chemicals occur in very small quantities, it has so far been difficult to develop a sufficiently reliable and robust apparatus suitable for operation at a sampling point in waterways or at sea.
The extraction devices known so far are only intended for use in laboratories. Manual extraction processes are extremely laborious and are not suitable for large quantities of water.
Attempts have also been made to separate these chemicals by filter-ing them t-hrough carbon filters, which enable a high degree o~
absorption, but have the drawback that the filtrate is altered after a short time so that it is no longer identical to the chemicals originally caught. Furthermore, it has proved difficult to extract the chemicals from the carbon filter. It is also known to use porous polyurethane foam as filtér, which has been found to be better than the carbon filter, but both these filters become clogged by particles in the water. This means, for instance, that it is difficult to check the water flow.
The object of the present invention is to provide an apparat-us which will eliminate the drawbacks mentioned above and which, due to its robust construct;on, can be used for field work and, due to its simple construction, can be looked after by an unquali-
~he increasing concentration of chemicals menacing the environment in our waterways necessitates substantially continuous supervision of the content of certain chemicals such as oil and chlorinated hydrocarbon, particularly polychlorinated biphenyls (PCB). The presence of such chemicals in lakes and rivers causes undesirable biological results, and careful supervision of their content is therefore necessary. Since these chemicals occur in very small quantities, it has so far been difficult to develop a sufficiently reliable and robust apparatus suitable for operation at a sampling point in waterways or at sea.
The extraction devices known so far are only intended for use in laboratories. Manual extraction processes are extremely laborious and are not suitable for large quantities of water.
Attempts have also been made to separate these chemicals by filter-ing them t-hrough carbon filters, which enable a high degree o~
absorption, but have the drawback that the filtrate is altered after a short time so that it is no longer identical to the chemicals originally caught. Furthermore, it has proved difficult to extract the chemicals from the carbon filter. It is also known to use porous polyurethane foam as filtér, which has been found to be better than the carbon filter, but both these filters become clogged by particles in the water. This means, for instance, that it is difficult to check the water flow.
The object of the present invention is to provide an apparat-us which will eliminate the drawbacks mentioned above and which, due to its robust construct;on, can be used for field work and, due to its simple construction, can be looked after by an unquali-
- 2 - ~
1()5;~538 field operator. It should also be possible to use the apparatus immersed below the surface of the water for separation in situ.
According to the present invention there is provided apparatus for extracting dissolved substances from water by means of a solvent, which comprises an extraction vessel; a stationary container, having side walls and a bottom but open at the top, arranged in the lower part of the extrac-tion vessel there being an annular gap between the side walls of the con-tainer and said vessel; said container having therein a stirrer, and acting as a mixing container; an inlet conduit for supplying solvent to the vessel;
an inlet conduit for supplying water to the container, where water is mixed with solvent in the extraction vessel; an outlet conduit for removing water from the bottom of the annular gap between the extraction vessel and the container; and means in said annular gap to reduce the turbulence caused by the stirring in the mixture of water and solvent moving down in said annular gap, so that the solvent rises to the upper part of the extraction vessel and only water is removed through the outlet conduit, said means for reduc-ing the turbulence in the annular gap comprising a partition provided with openings, which partition divides said gap into an upper section and a lower section.
In the accompanying drawings which illustrate two embodiments of the present invention:
Figure 1 shows a section through an extraction apparatus according to a first embodiment of the invention.
FiguTe 2 is a section along the line II-II in Figure 1.
Figure 3 is a section along the line III-III in Figure 1.
~ Figure 4 shows a second embodiment of the invention with the addition of a means for continuously examining the extract.
The extraction apparatus according to Figures 1-3 comprises an extraction vessel 1 consisting of a glass cylinder 2 having a lid 3 at the top and a bottom 4. Inside the extiaction vessel is a container 5, provided
1()5;~538 field operator. It should also be possible to use the apparatus immersed below the surface of the water for separation in situ.
According to the present invention there is provided apparatus for extracting dissolved substances from water by means of a solvent, which comprises an extraction vessel; a stationary container, having side walls and a bottom but open at the top, arranged in the lower part of the extrac-tion vessel there being an annular gap between the side walls of the con-tainer and said vessel; said container having therein a stirrer, and acting as a mixing container; an inlet conduit for supplying solvent to the vessel;
an inlet conduit for supplying water to the container, where water is mixed with solvent in the extraction vessel; an outlet conduit for removing water from the bottom of the annular gap between the extraction vessel and the container; and means in said annular gap to reduce the turbulence caused by the stirring in the mixture of water and solvent moving down in said annular gap, so that the solvent rises to the upper part of the extraction vessel and only water is removed through the outlet conduit, said means for reduc-ing the turbulence in the annular gap comprising a partition provided with openings, which partition divides said gap into an upper section and a lower section.
In the accompanying drawings which illustrate two embodiments of the present invention:
Figure 1 shows a section through an extraction apparatus according to a first embodiment of the invention.
FiguTe 2 is a section along the line II-II in Figure 1.
Figure 3 is a section along the line III-III in Figure 1.
~ Figure 4 shows a second embodiment of the invention with the addition of a means for continuously examining the extract.
The extraction apparatus according to Figures 1-3 comprises an extraction vessel 1 consisting of a glass cylinder 2 having a lid 3 at the top and a bottom 4. Inside the extiaction vessel is a container 5, provided
- 3 -~S;~538 with a peripheral flange 6 sealing against the inner wall of the glass cy-linder. The extraction vessel 1 is divided by the container 5 and flange 6 into an upper depositing zone A, a lower mixing zone B, an annular first separating chamber C and a second separating chamber D located below the first. The chambers C and D communicate with each other through openings 8 in the flange 6. The first separating chamber C has a cross-section which becomes wider towards the peripheral flange 6. The chamber C communicates with the zone A through an annular gap 7. The material used for the lid 3, bottom 4 and container 5 is a plastic such as polytetrafluorethylene which is resistant to the chemicals occurring.
The container 5 contains a rod-shaped stirring member 10 being placed freely at the bottom of the container 5. The stirring member 10 can be rotated by means of a magnetic stirrer 9, operated by a switch 38.
The lid 3 of the glass cylinder is provided with an inlet channel 11 for supplying the water to be extracted and a channel 12 which can be used for adding the solvent. The bottom plate 4 of the glass cylinder is provided with outlet openings 13 communicating through an annular groove 14 with an outlet channel 15.
The upper portion of the outer wall of the container 5 is provided with protruding portions 16, looking like saw-tooths in cross-section, thus giving the separating chamber C alternating wider and narrower sections, in order to reduce the liquid turbulence in this chamber C.
The apparatus according to Figures 1-3 functions in the following manner:
The extraction ~ssel 1 is filled to about one third of its volume with a solvent which will not mix with water, for example cyclohexane. The inlet channel 11 is connected to one end of a tube 17, the other end of which is placed in the water to be examined. A pump 19 is connected to the outlet channel 15 which, through a tube 18, draws the water through the apparatus. The reference character 37 in Figure 1 indicates the interface between i~S;~S38 the body 36 of water and the body 35 of solvent before the stirrer 9 has been started.
Upon starting the magnetic stirrer 9 the stirring member 10 produces vigorous stirring in the vessel 5 and the adjacent zone A
thus mixing the solvent with the water entering the apparatus to form a water-solvent emulsion. Chemicals in the water which can be extracted by the solvent are thus dissolved out of the water.
The stirrer 10 produces an eddy current which extends into the depositing ~one with gradually decreasing effect. Since the mix-ing ~one B is narrower, i.e. has a smaller cross-sectional area than the depositin~; zone, a less turbulent region is obtained just opposite the gap 7, where separation of the two liquid phases is initiated. Due to the suction force of the pump 19 the water-solvent emulsion flows into the first separation chamber C
where the turbulence of the liquid is further reduced and continu-ed separation of the lighter solvent from the extracted water takes place. Because of the difference in density, the lighter solvent will rise to the depositin~ zone A where the two liquids wiil separate into layers. From the first separation chamber C
the water, together with a small quantity of solvent,will reach the second separating chamber D where the flow of water is sub-stantially laminar and any remaining d~oplets of solvent will flow upwardly through the holes 8. The extracted water, which does not contain any solvent droplets, leaves the apparatus through the outlet channel 15.
It will be understood t~lat the entire quantity of solvent remains in the apparatus during the whole extraction process.
When the desired quantity of water has passed through the apparat-us the extraction operation ;s discontinued, the solvent is remov-l30 ed from the apparatus, and ;ts content of' substance extracted ~ l - --lOS~S3~ ~
from the water is analyzed. This analysis of course depends on the nature of` the substance. The analysis does not form part of this invention, and will not be described here.
For an apparatus having the dimensions shol~m in Fig. 1 a flow rate of 1-10 litres of water per hour has been found suit-able, the quantity of solvent (cyclohexane) being 250 ml. The apparatus according to the invention has enable~ a concentration of poly-chlorinated biphenyl as low as 0.2 ng per litre of water to be analyzed.
In Fig. 4 the same reference characters as in Figs. 1-3 have been used for equivalent parts. The apparatus according to Fig. ~ contains an external circulation conduit 24 containing means 25 for the continuous photometric analysis of the solvent.
The solvent is circulated by means of a pump 46. A collar-~haped partition 27 is provided in the upper portion of the zone A to separate the two ends of the conduit 24 and to reduce the turbul-ence in the zone A. A propeller ~3, driven by a motor 44, in the zone B mixes the two liquids to produce the water-solvent emulsior .
The separating chambers C and D are separated by a wall 45 con-taining the openings 8. The apparatus makes it possible to as-certain continuously, in the course of the extraction process, the amount of substance having been tr,ansferred from the water to the solvent.
The container 5 contains a rod-shaped stirring member 10 being placed freely at the bottom of the container 5. The stirring member 10 can be rotated by means of a magnetic stirrer 9, operated by a switch 38.
The lid 3 of the glass cylinder is provided with an inlet channel 11 for supplying the water to be extracted and a channel 12 which can be used for adding the solvent. The bottom plate 4 of the glass cylinder is provided with outlet openings 13 communicating through an annular groove 14 with an outlet channel 15.
The upper portion of the outer wall of the container 5 is provided with protruding portions 16, looking like saw-tooths in cross-section, thus giving the separating chamber C alternating wider and narrower sections, in order to reduce the liquid turbulence in this chamber C.
The apparatus according to Figures 1-3 functions in the following manner:
The extraction ~ssel 1 is filled to about one third of its volume with a solvent which will not mix with water, for example cyclohexane. The inlet channel 11 is connected to one end of a tube 17, the other end of which is placed in the water to be examined. A pump 19 is connected to the outlet channel 15 which, through a tube 18, draws the water through the apparatus. The reference character 37 in Figure 1 indicates the interface between i~S;~S38 the body 36 of water and the body 35 of solvent before the stirrer 9 has been started.
Upon starting the magnetic stirrer 9 the stirring member 10 produces vigorous stirring in the vessel 5 and the adjacent zone A
thus mixing the solvent with the water entering the apparatus to form a water-solvent emulsion. Chemicals in the water which can be extracted by the solvent are thus dissolved out of the water.
The stirrer 10 produces an eddy current which extends into the depositing ~one with gradually decreasing effect. Since the mix-ing ~one B is narrower, i.e. has a smaller cross-sectional area than the depositin~; zone, a less turbulent region is obtained just opposite the gap 7, where separation of the two liquid phases is initiated. Due to the suction force of the pump 19 the water-solvent emulsion flows into the first separation chamber C
where the turbulence of the liquid is further reduced and continu-ed separation of the lighter solvent from the extracted water takes place. Because of the difference in density, the lighter solvent will rise to the depositin~ zone A where the two liquids wiil separate into layers. From the first separation chamber C
the water, together with a small quantity of solvent,will reach the second separating chamber D where the flow of water is sub-stantially laminar and any remaining d~oplets of solvent will flow upwardly through the holes 8. The extracted water, which does not contain any solvent droplets, leaves the apparatus through the outlet channel 15.
It will be understood t~lat the entire quantity of solvent remains in the apparatus during the whole extraction process.
When the desired quantity of water has passed through the apparat-us the extraction operation ;s discontinued, the solvent is remov-l30 ed from the apparatus, and ;ts content of' substance extracted ~ l - --lOS~S3~ ~
from the water is analyzed. This analysis of course depends on the nature of` the substance. The analysis does not form part of this invention, and will not be described here.
For an apparatus having the dimensions shol~m in Fig. 1 a flow rate of 1-10 litres of water per hour has been found suit-able, the quantity of solvent (cyclohexane) being 250 ml. The apparatus according to the invention has enable~ a concentration of poly-chlorinated biphenyl as low as 0.2 ng per litre of water to be analyzed.
In Fig. 4 the same reference characters as in Figs. 1-3 have been used for equivalent parts. The apparatus according to Fig. ~ contains an external circulation conduit 24 containing means 25 for the continuous photometric analysis of the solvent.
The solvent is circulated by means of a pump 46. A collar-~haped partition 27 is provided in the upper portion of the zone A to separate the two ends of the conduit 24 and to reduce the turbul-ence in the zone A. A propeller ~3, driven by a motor 44, in the zone B mixes the two liquids to produce the water-solvent emulsior .
The separating chambers C and D are separated by a wall 45 con-taining the openings 8. The apparatus makes it possible to as-certain continuously, in the course of the extraction process, the amount of substance having been tr,ansferred from the water to the solvent.
Claims (3)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. Apparatus for extracting dissolved substances from water by means of a solvent, which comprises an extraction vessel;
a stationary container, having side walls and a bottom but open at the top, arranged in the lower part of the extraction vessel there being an annular gap between the side walls of the container and said vessel;
said container having therein a stirrer, and acting as a mixing con-tainer;
an inlet conduit for supplying solvent to the vessel;
an inlet conduit for supplying water to the container, where water is mixed with solvent in the extraction vessel;
an outlet conduit for removing water from the bottom of the annular gap between the extraction vessel and the container; and means in said annular gap to reduce the turbulence caused by the stir-ring in the mixture of water and solvent moving down in said annular gap, so that the solvent rises to the upper part of the extraction vessel and only water is removed through the outlet conduit.
said means for reducing the turbulence in the annular gap comprising a partition provided with openings, which partition divides said gap into an upper section and a lower section.
a stationary container, having side walls and a bottom but open at the top, arranged in the lower part of the extraction vessel there being an annular gap between the side walls of the container and said vessel;
said container having therein a stirrer, and acting as a mixing con-tainer;
an inlet conduit for supplying solvent to the vessel;
an inlet conduit for supplying water to the container, where water is mixed with solvent in the extraction vessel;
an outlet conduit for removing water from the bottom of the annular gap between the extraction vessel and the container; and means in said annular gap to reduce the turbulence caused by the stir-ring in the mixture of water and solvent moving down in said annular gap, so that the solvent rises to the upper part of the extraction vessel and only water is removed through the outlet conduit.
said means for reducing the turbulence in the annular gap comprising a partition provided with openings, which partition divides said gap into an upper section and a lower section.
2. Apparatus according to claim 1, characterized in that a pump is connected to the outlet conduit in order to draw water through the apparatus.
3. Apparatus according to claim 1, characterized in that the means for reducing the turbulence in the gap further includes protruding parts on the wall of the upper part of the annular gap.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA219,738A CA1052538A (en) | 1975-02-10 | 1975-02-10 | Apparatus for continuous liquid-liquid extraction of water with a solvent |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA219,738A CA1052538A (en) | 1975-02-10 | 1975-02-10 | Apparatus for continuous liquid-liquid extraction of water with a solvent |
Publications (1)
Publication Number | Publication Date |
---|---|
CA1052538A true CA1052538A (en) | 1979-04-17 |
Family
ID=4102251
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA219,738A Expired CA1052538A (en) | 1975-02-10 | 1975-02-10 | Apparatus for continuous liquid-liquid extraction of water with a solvent |
Country Status (1)
Country | Link |
---|---|
CA (1) | CA1052538A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3056257A1 (en) * | 2014-11-25 | 2016-08-17 | Fidica GmbH & Co. KG | Monitoring of ro installation for flush solutions |
-
1975
- 1975-02-10 CA CA219,738A patent/CA1052538A/en not_active Expired
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3056257A1 (en) * | 2014-11-25 | 2016-08-17 | Fidica GmbH & Co. KG | Monitoring of ro installation for flush solutions |
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